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Designation: E1461 13

Standard Test Method for


Thermal Diffusivity by the Flash Method1
This standard is issued under the fixed designation E1461; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon () indicates an editorial change since the last revision or reapproval.

1. Scope 2. Referenced Documents


1.1 This test method covers the determination of the thermal 2.1 ASTM Standards:2
diffusivity of primarily homogeneous isotropic solid materials. C714 Test Method for Thermal Diffusivity of Carbon and
Thermal diffusivity values ranging from 0.1 to 1000 (mm)2 s-1 Graphite by Thermal Pulse Method
are measurable by this test method from about 75 to 2800 K. E228 Test Method for Linear Thermal Expansion of Solid
1.2 Practice E2585 is adjunct to this test method and Materials With a Push-Rod Dilatometer
contains detailed information regarding the use of the flash E2585 Practice for Thermal Diffusivity by the Flash Method
method. The two documents are complementing each other.
3. Terminology
1.3 This test method is a more detailed form of Test Method
3.1 Definitions of Terms Specific to This Standard:
C714, having applicability to much wider ranges of materials,
3.1.1 thermal conductivity, , of a solid materialthe time
applications, and temperatures, with improved accuracy of
rate of steady heat flow through unit thickness of an infinite
measurements.
slab of a homogeneous material in a direction perpendicular to
1.4 This test method is intended to allow a wide variety of the surface, induced by unit temperature difference. The
apparatus designs. It is not practical in a test method of this property must be identified with a specific mean temperature,
type to establish details of construction and procedures to cover since it varies with temperature.
all contingencies that might offer difficulties to a person
3.1.2 thermal diffusivity, , of a solid materialthe property
without pertinent technical knowledge, or to restrict research
given by the thermal conductivity divided by the product of the
and development for improvements in the basic technique.
density and heat capacity per unit mass.
1.5 This test method is applicable to the measurements
3.2 Description of Symbols and Units Specific to This
performed on essentially fully dense (preferably, but low
Standard:
porosity would be acceptable), homogeneous, and isotropic
3.2.1 Ddiameter, m.
solid materials that are opaque to the applied energy pulse.
Experience shows that some deviation from these strict guide- 3.2.2 Cpspecific heat capacity, Jg-1K-1.
lines can be accommodated with care and proper experimental 3.2.3 kconstant depending on percent rise.
design, substantially broadening the usefulness of the method. 3.2.4 Kcorrection factors.
1.6 The values stated in SI units are to be regarded as 3.2.5 K1, K2constants depending on .
standard. No other units of measurement are included in this 3.2.6 Lspecimen thickness, mm.
standard.
3.2.7 tresponse time, s.
1.7 For systems employing lasers as power sources, it is
imperative that the safety requirement be fully met. 3.2.8 t1/2half-rise time or time required for the rear face
temperature rise to reach one half of its maximum value, s.
1.8 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.2.9 t*dimensionless time (t* = 4s t/DT2).
responsibility of the user of this standard to establish appro- 3.2.10 Ttemperature, K.
priate safety and health practices and determine the applica- 3.2.11 thermal diffusivity, (mm)2/s.
bility of regulatory limitations prior to use. 3.2.12 fraction of pulse duration required to reach maxi-
mum intensity.
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.05 on Thermo-
2
physical Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2013. Published October 2013. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1992. Last previous edition approved in 2011 as E1461 11. DOI: Standards volume information, refer to the standards Document Summary page on
10.1520/E1461-13. the ASTM website.

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E1461 13
3.2.13 density, g/(cm)3.
3.2.14 thermal conductivity, Wm-1K-1.
3.2.15 t5T(5t ) /T(t ).
12 12

3.2.16 t10T(10t ) /T(t ).


12 12

3.2.17 Tmaxtemperature difference between baseline and


maximum rise, K.
3.2.18 pulse duration (see Fig. 1).
3.3 Description of Subscripts Specific to This Standard:
FIG. 2 Schematic of the Flash Method
3.3.1 xpercent rise.
3.3.2 Rratio.
3.3.3 maxmaximum.
3.3.4 pconstant pressure.

4. Summary of Test Method


4.1 A small, thin disc specimen is subjected to a high-
intensity short duration radiant energy pulse (Fig. 2). The
energy of the pulse is absorbed on the front surface of the
specimen and the resulting rear face temperature rise (thermal
curve) is recorded. The thermal diffusivity value is calculated
from the specimen thickness and the time required for the rear
face temperature rise to reach a percentage of its maximum FIG. 3 Characteristic Thermal Curve for the Flash Method
value (Fig. 3). When the thermal diffusivity of the specimen is
to be determined over a temperature range, the measurement 5.2 The flash method is used to measure values of thermal
must be repeated at each temperature of interest. diffusivity, , of a wide range of solid materials. It is particu-
larly advantageous because of simple specimen geometry,
NOTE 1This test method is described in detail in a number of
publications (1, 2)3 and review articles (3, 4, 5). A summary of the theory small specimen size requirements, rapidity of measurement
can be found in Appendix X1. and ease of handling.
5.3 Under certain strict conditions, specific heat capacity of
5. Significance and Use
a homogeneous isotropic opaque solid specimen can be deter-
5.1 Thermal diffusivity is an important transient thermal mined when the method is used in a quantitative fashion (see
property, required for such purposes such as design Appendix X2).
applications, determination of safe operating temperature,
5.4 Thermal diffusivity results, together with related values
process control, and quality assurance.
of specific heat capacity (Cp) and density () values, can be
used in many cases to derive thermal conductivity (), accord-
ing to the relationship:
3
5 Cp (1)
The boldface numbers given in parentheses refer to a list of references at the
end of the text.
6. Interferences
6.1 In principle, the thermal diffusivity is obtained from the
thickness of the specimen and from a characteristic time
function describing the propagation of heat from the front
surface of the specimen to its back surface. The sources of
uncertainties in the measurement are associated with the
specimen itself, the temperature measurements, the perfor-
mance of the detector and of the data acquisition system, the
data analysis and more specifically the finite pulse time effect,
the nonuniform heating of the specimen and the heat losses
(radiative and conductive). These sources of uncertainty can be
considered systematic, and should be carefully considered for
each experiment. Errors random in nature (noise, for example)
FIG. 1 Laser Pulse Shape can be best estimated by performing a large number of repeat

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E1461 13
experiments. The relative standard deviation of the obtained 7.5 Data Recording:
results is a good representation of the random component of the 7.5.1 The data acquisition system must be of an adequate
uncertainty associated with the measurement. Guidelines in speed to ensure that resolution in determining half-rise time on
performing a rigorous evaluation of these factors are given in the thermal curve is no more than 1 % of the half-rise time, for
(6). the fastest thermal curve for which the system is qualified.
7. Apparatus 7.6 Measurement of specimens temperature is performed
The essential components of the apparatus are shown in Fig. using calibrated temperature sensors such as a thermocouple,
4. These are the flash source, specimen holder, environmen- optical pyrometer, platinum resistance temperature detector
tal enclosure (optional), temperature detector and recording (RTD), etc. The temperature sensor shall be in intimate contact
device. with or trained on the sample holder, in close proximity of the
specimen.
7.1 The flash source may be a pulse laser, a flash lamp, or
other device capable to generate a short duration pulse of NOTE 3Touching the specimen with thermocouples is not recom-
mended. Embedding thermocouples into the specimen is not acceptable.
substantial energy. The duration of the pulse should be less
than 2 % of the time required for the rear face temperature rise 7.7 The temperature controller and/or programmer are to
to reach one half of its maximum value (see Fig. 3). bring the specimen to the temperatures of interest.
NOTE 2A pulse length correction may be applied (7, 8, 9) permitting 8. Test Specimen
use of pulse durations greater than 0.5 %.
8.1 The usual specimen is a thin circular disc with a front
7.1.1 The energy of the pulse hitting the specimens surface
surface area less than that of the energy beam. Typically,
must be spatially uniform in intensity.
specimens are 10 to 12.5 mm in diamete (in special cases, as
7.2 An environmental control chamber is required for mea- small as 6 mm diameter and as large as 30 mm diameter have
surements above and below room temperature. been reported as used successfully). The optimum thickness
7.3 The temperature detector can be a thermocouple, infra- depends upon the magnitude of the estimated thermal
red detector, optical pyrometer, or any other sensor that can diffusivity, and should be chosen so that the time to reach half
provide a linear electrical output proportional to a small of the maximum temperature falls within the 10 to 1000 ms
temperature rise. It shall be capable of detecting 0.05 K change range. Thinner specimens are desired at higher temperatures to
above the specimens initial temperature. The detector and its minimize heat loss corrections; however, specimens should
associated amplifier must have a response time not more than always be thick enough to be representative of the test material.
2 % of the half-rise time value. Typically, thicknesses are in the 1 to 6 mm range.
7.4 The signal conditioner includes the electronic circuit to 8.2 Specimens must be prepared with faces flat and parallel
bias out the ambient temperature reading, spike filters, within 0.5 % of their thickness, in order to keep the error in
amplifiers, and analog-to-digital converters. thermal diffusivity due to the measured average thickness, to
less than 1 %. Non-uniformity of either surface (craters,
scratches, markings) should be avoided
8.3 Specimen Surface PreparationIt is a good practice to
apply a very thin, uniform graphite or other high emissivity
coating on both faces of the specimen to be tested, prior to
performing the measurements. The coating may be applied by
spraying, painting, sputtering, etc. This will improve the
capability of the specimen to absorb the energy applied,
especially in case of highly reflective materials. For transparent
materials, a layer of gold, silver, or other opaque materials
must be deposited first, followed by graphite coating. For some
opaque reflective materials, grit blasting of the surface can
provide sufficient pulse absorption and emissivity, especially at
higher temperatures, where coatings may not be stable or may
react with the material.

9. Calibration and Verification


9.1 It is important to periodically verify the performance of
a device and to establish the extent these errors may affect the
data generated. This can be accomplished by testing one or
several materials whose thermal diffusivity is well known (see
Appendix X3).
9.1.1 The use of reference materials to establish validity of
the data on unknown materials can lead to unwarranted
FIG. 4 Block Diagram of a Flash System statements on accuracy. The use of references is only valid

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E1461 13
when the properties of the reference (including half-rise times 5 0.13879 L 2 /t (2)
and thermal diffusivity values) are similar to those of the
Check the validity of the experiment by calculating at a
unknown and the temperature-rise curves are determined in an
minimum of two other points on the rise curve. The equation is
identical manner for the reference and unknown.
as follows:
9.1.2 An important check of the validity of data (in addition
to the comparison of the rise curve with the theoretical model), 5 k x L 2 /t x (3)
when corrections have been applied, is to vary the specimen where:
thickness. Since the half times vary as L2, decreasing the
tx = the time required for the temperature rise to reach x
specimen thickness by one-half should decrease the half time
percent of Tmax. Values of kx are given in Table 1.
to one-fourth of its original value. Thus, if one obtains the same
thermal diffusivity value (appropriate heat loss corrections 11.1.1 Ideally, the calculated values of for different values
being applied) with representative specimens from the same of x should all be the same. If the values at 25, 50 and 75 %
material of significantly different thicknesses, the results can be Tmax lie within 62 %, the overall accuracy is probably within
assumed valid. 65 % at the half-rise time. If the values lie outside of this
range, the response curve should be analyzed further to see if
10. Procedure thermal radiation heat loss, finite-pulse time or non-uniform
10.1 For commercially produced systems, follow manufac- heating effects are present.
turers instructions. 11.1.2 Thermal radiation heat loss effects are most readily
determined from the temperature of the specimen and the
10.2 The testing procedure must contain the following rear-face temperature response after 4t1/2 by plotting the
functions: experimental values of T/Tmax versus t/t1/2 along with the
10.2.1 Determine and record the specimen thickness. values for the theoretical model. Some numbers for the
10.2.2 Mount the specimen in its holder. theoretical model are given in Table 2.
10.2.3 Establish vacuum or inert gas environment in the 11.1.3 Prepare a display of the normalized experimental
chamber if necessary. data and the theoretical model using the tabulated values of
10.2.4 Determine specimen temperature unless the system T/Tmax and t/t1/2 and the corresponding experimental data at
will do it automatically. several percent levels of the rise. All normalized experimental
10.2.5 Especially at low temperatures, use the lowest level curves must pass through T/Tmax = 0.5 and t/t1/2 = 1.0.
of power for the energy pulse able to generate a measurable Calculations including the 25 to 35 % and 65 to 80 % ranges
temperature rise, in order to ensure that the detector functions are required to compare the experimental data with the
within its linear range. theoretical curve.
10.2.6 After the pulse delivery, monitor the raw or pro- 11.1.4 Examples of the normalized plots for experiments
cessed thermal curve to establish in-range performance. In case that approximate the ideal case, in which both radiation heat
of multiple specimen testing, it is advisable (for time economy) losses and finite pulse time effect exist, are shown in Figs. 5
to sequentially test specimens at the same temperature (includ- and 6, and Fig. 7. Various procedures for correcting for these
ing replicate tests) before proceeding to the next test tempera- effects are also given in Refs. (4, 7-13) and specific examples
ture. are given in 11.2 and 11.3.
10.2.7 The temperature stability (base line) prior and during 11.1.5 The corrections can be minimized by the proper
a test shall be verified either manually or automatically to be selection of specimen thickness. The finite pulse time effect
less than 4 % of the maximum temperature rise. decreases as the thickness is increased, while heat losses
NOTE 4Testing during the temperature program is not recommended decrease as the thickness is reduced.
as it results in lower precision. 11.1.6 Non-uniform heating effects also cause deviations of
10.2.8 Determine the specimen ambient temperature and the reduced experimental curve from the model because of
collect the base line, transient-rise and cooling data, and two-dimensional heat flow. Since there are a variety of non-
analyze the results according to Section 11. uniform heating cases, there are a variety of deviations. Hot
10.2.9 Change or program the specimen temperature as center cases approximate the radiation heat loss example. Cold
desired and repeat the data collection process to obtain center cases result in the rear face temperature continuing to
measurements at each temperature. rise significantly after 4t1/2. Non-uniform heating may arise
10.2.10 If required, repeat the measurements at each tem- from the nature of the energy pulse or by non-uniform
perature on the specimens cooling or on its re-heating over the
same cycle.
TABLE 1 Values of the Constant kx for Various Percent Rises
11. Calculation x(%) kx x(%) kx

11.1 Determine the baseline and maximum rise to give the 10 0.066108 60 0.162236
20 0.084251 66.67 0.181067
temperature difference, Tmax. Determine the time required 25 0.092725 70 0.191874
from the initiation of the pulse for the rear face temperature to 30 0.101213 75 0.210493
reach half Tmax. This is the half-rise time, t1/2. Calculate the 33.33 0.106976 80 0.233200
40 0.118960 90 0.303520
thermal diffusivity, , from the specimen thickness, L, and the 50 ... ... ...
half-rise time t1/2, as follows (1):

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E1461 13
TABLE 2 Values of Normalized Temperature Versus Time for
Theoretical Model
T/Tmax t/t
12 T/Tmax t/t
12

0 0 0.7555 1.5331
0.0117 0.2920 0.7787 1.6061
0.1248 0.5110 0.7997 1.6791
0.1814 0.5840 0.8187 1.7521
0.2409 0.6570 0.8359 1.8251
0.3006 0.7300 0.8515 1.8981
0.3587 0.8030 0.8656 1.9711
0.4140 0.8760 0.8900 2.1171
0.4660 0.9490 0.9099 2.2631
0.5000 1.0000 0.9262 2.4091
0.5587 1.0951 0.9454 2.6281
0.5995 1.1681 0.9669 2.9931
0.6369 1.2411 0.9865 3.6502
0.6709 1.3141 0.9950 4.3802
0.7019 1.3871 0.9982 5.1102
0.7300 1.4601 ... ... FIG. 7 Normalized Rear Face Temperature Rise: Comparison of
Mathematical Model (No Heat Loss) to Experimental Values with
Radiation Heat Losses

For this to be valid, the evolution of the pulse intensity must


be representable by a triangle of duration and time to
maximum intensity of as shown in Fig. 1. The pulse shape
for the laser may be determined using an optical detector. From
the pulse shape so determined, and are obtained. Values of
the two constants K1 and K2 for various values of are given
in Table 3 for correcting x.
11.3 Heat loss corrections can be performed using proce-
dures proposed in a (12, 13), for example. Both of these
corrections are affected by non-uniform heating effects. Cor-
rections given in (12) by Cowan are affected by conduction
heat losses to the holders in addition to the radiation heat losses
FIG. 5 Comparison of Non-dimensionalized Temperature Re- from the specimen surfaces. Thus, the errors in the correction
sponse Curve to Mathematical Model procedures are affected by different physical phenomena and a
comparison of thermal diffusivity values corrected by the two
procedures is useful in determining the presence or absence of
these phenomena.
11.3.1 Determine the ratio of the net rise time values at
times that are five and ten times the experimental half-rise time
value to the net rise at the half-rise time value (12). These ratios
are designated as t5 and t10. If there are no heat losses t5
= t10 = 2.0. The correction factors (KC ) for the five and ten
half-rise time cases are calculated from the polynomial fits:
K C 5 A1B ~ t ! 1C ~ t ! 2 1D ~ t ! 3 1E ~ t ! 4 (5)

1F ~ t ! 5 1G ~ t ! 6 1H ~ t ! 7

where:
values for the coefficients A through H are given in Table 4.
FIG. 6 Normalized Rear Face Temperature Rise: Comparison of Corrected values for thermal diffusivity are calculated from the
Mathematical Model (No Finite Pulse Time Effect) to Experimen- following relation:
tal Values with Finite Pulse Time
corrected 5 0.5 K C /0.13885 (6)

absorption on the front surface of the specimen. The former


case must be eliminated by altering the energy source, while TABLE 3 Finite Pulse Time Factors
the latter may be eliminated by adding an absorbing layer and K1 K2
using two-layer mathematics (4, 14). 0.15 0.34844 2.5106
0.28 0.31550 2.2730
11.2 Finite pulse time effects usually can be corrected for 0.29 0.31110 2.2454
using the equation: 0.30 0.30648 2.2375
0.50 0.27057 1.9496
5 K 1 L 2/ ~ K 2 t x 2 ! (4)

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E1461 13
TABLE 4 Coefficients for Cowan Corrections 12.2.1 Statement that the response time of the detector,
Coefficients Five Half Times Ten Half Times including the associated electronics was adequately checked,
A 0.1037162 0.054825246 and the method used;
B 1.239040 0.16697761
C 3.974433 0.28603437
12.2.2 Energy pulse source;
D 6.888738 0.28356337 12.2.3 Beam uniformity;
E 6.804883 0.13403286
F 3.856663 0.024077586 12.2.4 Type of temperature detector;
G 1.167799 0.0 12.2.5 Manufacturer and model of the instrument used;
H 0.1465332 0.0
12.2.6 Dated version of this test method used.

13. Precision and Bias


where:
0.5 = the uncorrected thermal diffusivity value calculated 13.1 The precision and bias information for this standard are
using the experimental half-rise time. obtained from literature meta-analysis performed in 2013. The
results of study are on file at ASTM Headquarters.4
11.3.2 Heat loss corrections based on the procedure given in
Clark and Taylor (12) also use ratio techniques. For the 13.2 Precision:
t0.75/t0.25 ratio, that is, the time to reach 75 % of the maximum 13.2.1 Within laboratory variability may be described using
divided by the time to reach 25 % of the maximum, the ideal the repeatability value (r) obtained by multiplying the repeat-
value is 2.272. Determine this ratio from the experimental data. ability standard deviation by 2.8. The repeatability value
Then calculate the correction factor (KR) from the following estimates the 95 % confidence limit. That is, two results from
equation: the same laboratory should be considered suspect (at the 95 %
K R 5 20.346146710.361578 ~ t 0.75/t 0.25! (7) confidence level) if they differ by more than the repeatability
value.
20.06520543 ~ t /t 0.25 ! 2
0.75 13.2.1.1 The within laboratory repeatability relative stan-
dard deviation from results obtained at 673 and 870 K is 2.0 %.
The corrected value for the thermal diffusivity at the half-rise
time is corrected = 0.5 KR /0.13885. Corrections based on 13.2.1.2 The within laboratory repeatability relative stan-
many other ratios can also be used. dard deviation is reported in the literature to be temperature
dependent and to decrease with increasing temperature (15).
11.4 If the measurements are performed at temperatures
13.2.2 Between laboratory variability may be described
different from that where the specimen thickness has been
using the reproducibility value (R) obtained by multiplying the
determined, consider the presence of the linear thermal expan-
reproducibility standard deviation by 2.8. The reproducibility
sion effects. If these effects are not negligible, calculate the
value estimates the 95 % confidence limit. That is, results
specimen thickness at each temperature and apply the usual
obtained in two different laboratories should be considered
procedure as described above.
suspect (at the 95 % confidence level) if they differ by more
11.5 Other parameter estimation methods may also be used, than the reproducibility value.
provided detailed reference to the source is reported with the 13.2.2.1 The between laboratory reproducibility standard
data. deviation from results obtained at 673 K is 13 % and at 870 K
is 8.1 %.
12. Report
13.2.2.2 The between laboratory reproducibility standard
12.1 The report shall contain: deviation is observed to be temperature dependent and to
12.1.1 Identification of the specimen (material) and previ- decrease with increasing temperature (15).
ous history;
12.1.2 Specimen thickness, m; 13.3 Bias:
12.1.3 Temperature, C; 13.3.1 Bias is the difference between the mean value ob-
12.1.4 Calculated value of thermal diffusivity at x = 50 %, at tained and an accepteble reference value for the same material.
the reported temperature; 13.3.2 The mean value for the thermal diffusivity for
12.1.5 Calculated values near x = 25 and 75 % as well as x AXM-5Q graphite was found to be 0.259 cm2/s at 673 K and
= 50 %, or a comparison of the reduced experimental curve to 0.208 cm2/s at 870 K. The best estimate literature value for
the model, at each temperature; AXM-5Q graphite at these temperatures are 0.279 and 0.208
12.1.6 Repeatability of results at each temperature; cm2/s, respectively representing -7.7 % and 0 % bias at these
12.1.7 Whether or not the data was corrected for thermal temperatures.
expansion. If this correction was made, the thermal expansion 13.3.3 Bias is observed to be temperature dependent and to
values used must be reported; decrease with increasing temperature (15).
12.1.8 Description of any correction procedures for heat
loss and finite pulse length effect.
12.1.9 Environmental surroundings of the specimen (gas
4
type, pressure, etc.). Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:E37-1043. Contact ASTM Customer
12.2 Additionally, it is beneficial to report: Service at service@astm.org.

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E1461 13
14. Keywords
14.1 flash method; infrared detectors; intrinsic thermo-
couples; specific heat capacity; thermal conductivity; thermal
diffusivity; transient temperature measurements

APPENDIXES

X1. THEORY

X1.1 The Ideal CaseThe physical model of the pulse At the rear surface, where x = L, the temperature history can
method is founded on the thermal behavior of an adiabatic be expressed by:
(insulated) slab of material, initially at constant temperature,
whose one side has been subjected to a short pulse of energy.
The model assumes:
T ~ L,t ! 5
Q
CL F `

n51
(
112 ~ 21 ! n exp
2n 2 2
L
t S DG (X1.6)
Two dimensionless parameters, V and can be defined:
one dimensional heat flow; T ~ L,t !
no heat losses from the slabs surfaces; V ~ L,t ! 5 (X1.7)
TM
uniform pulse absorption at the front surface; 2 t
infinitesimally short pulse duration; 5
L2
(X1.8)
absorption of the pulse energy in a very thin layer; TM represents the maximum temperature at the rear surface.
homogeneity and isotropy of the slab material; The combination of Eq X1.6-X1.8 yields:
property invariance with temperature within experimental `
conditions. V 5 112 ( ~ 21 ! exp~ 2n
n 2
! (X1.9)
n51
In deriving the mathematical expression from which the
When V = 0.5, = 1.38, and therefore:
thermal diffusivity is calculated, Parker (1) starts from the
equation of the temperature distribution within a thermally 1.38L 2
5 (X1.10)
insulated solid of uniform thickness L, as given by Carslaw and 2t 1
2
Jaeger (16): or:
1 L L2
T ~ x,t ! 5
L * T ~ x,0 ! dx
0
5 0.1388
t1
(X1.11)
2

1
2 `
(
L n51
exp S
2n 2 2 t
L2 D
cos
n x
L * T ~ x,0 ! cos n Lx dx
0
L where t is the time required for the back surface to reach
12

half of the maximum temperature rise. A pulse experiment is


(X1.1) schematicallyis represented in Fig. 2.
where is the thermal diffusivity of the material. If a pulse As a result, a characteristic thermal curve of the rear face is
of radiant energy Q is instantaneously and uniformly absorbed created (Fig. 3).
in the small depth g at the front surface x = 0, the temperature
X1.2 The Non-Ideal CaseThe inadequacy of the Parker
distribution at that instant is given by
solution became obvious almost immediately after its
Q introduction, as nearly every one of these assumptions is
T ~ x,0 ! 5 (X1.2)
Cg violated to some extent during an experiment. So, gradually,
for 0 < x < g investigators introduced various theories to describe the real
and process, and solutions describing corrections to counter the
T ~ x,0 ! 5 0 (X1.3) violation of each of the boundary conditions. The ideal
for g < x < L. correction would encompass all factors present, but to date, no
With this initial condition, Eq X1.1 can be written as: such general correction has been developed. Instead, individual
or paired corrections accounting for deviations were intro-
n g
duced. The result is that one may end up with an array of

3 4
sin
T ~ x,0 ! 5
Q
CL
`

112 cos
n51
n x
L ( n g
L
exp S
2n 2 2
L2
t D numbers that vary substantially after using these corrections.
This is understandable, as historically, each investigator has
L
focused on one or another deviation from the ideal model,
(X1.4) while assuming ideality and constancy of the others. This by
where is the density and C is the specific heat capacity of itself is a substantial violation of principles, as in reality all
the material. In this application only a few terms will be parameters vary concurrently, in an extent dictated by the
needed, and since g is a very small number for opaque particular conditions of the experiment. Some situations may
materials, aggravate one condition, for example having a long pulse,
n g n g others may introduce other deviations, such as excessive heat
sin ' (X1.5)
L L losses from the front face due to using very powerful pulses,

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etc. It is therefore incumbent to choose the most proper ably from the one obtained with uniform irradiation. This effect
correction in harmony with the conditions of the experiment can be reduced by increasing the ratio between the specimens
analyzed. thickness and its radius. The same result can be achieved by
The finite pulse width effect, for example, occurs strongly using a temperature measurement system, which automatically
when thin specimens of high thermal diffusivity are tested (2, integrates the signal obtained from the rear face of the
8, 9, 17, 18), while the radiative heat losses become dominant specimen.
at high temperatures (12), when testing thick specimens. In It is a very difficult task to choose the best correction, and
contrast, nonuniform heating can occur during any thermal often not enough information is known about the equipment
diffusivity experiment (19). This can occur when a circular and the testing parameters to do it prudently. In principle, one
surface smaller than the specimen itself is irradiated, or the flux must return to the original premise: the accuracy of the data
density of the pulse varies from point-to-point over the depends on the agreement between the mathematical and
specimens surface. For the same amount of absorbed energy, experimental models. The purpose of applying corrections to
the dimensionless half-max time of the resulting thermal curve the experimental data is to bring it to closer agreement with the
at the center of the rear face of the specimen differs consider- ideal solution by accounting for the aberrations.

X2. MEASUREMENT OF SPECIFIC HEAT CAPACITY AND CALCULATION OF THERMAL CONDUCTIVITY

X2.1 The fundamental relationship between thermal diffu- X2.1.4 Both reference and unknown specimen must be
sivity (), thermal conductivity (), specific heat capacity (Cp), homogeneous and isotropic, as Eq X2.1 only applies for those
and density (), materials. Heterogeneous and anisotropic materials will fre-
quently produce erroneous data. The process is not purely

5 (X2.1) calorimetric, since the maximum temperature rise is derived
C p
from the signal provided largely by the components with the
allows the calculation of thermal conductivity, a much highest thermal diffusivity, while the internal equilibration may
sought after property, with the knowledge of the other proper- take place after that point in time. For this reason, this method
ties. A method was developed (1) where the specific heat tends to give erroneous results for specific heat capacity for
capacity of a specimen is determined when the thermal materials with large anisotropy (typically composites with an
diffusivity test is performed in a quantitative fashion. Caution ordered directional structure) and for mixtures of components
shall be used in performing this extenstion as errors abounds. with greatly differing thermal diffusivities.
In the course of an ordinary thermal diffusivity test, the amount X2.1.5 The reference and the unknown must be tested very
of energy is important only to the extent that it will generate a close to each other, both temporally (preferably only minutes
sufficient rear face signal. For operating in a calorimetric mode, apart) and thermally (strictly at the same temperature, in the
the energy level must be known closely, controllable and same environment).
repeatable. Approximating adiabatic conditions, the laser pulse
and the detector can be calibrated in unison when a specimen X2.1.6 This being a differential measurement, it is highly
of known specific heat capacity is tested. The measurement desirable to have both reference and unknown tested side-by-
will yield thermal diffusivity, and also a relative measure of side and with very small time intervals in between. It is also
energy expressed in terms of the absolute value of the desirable to test standard/specimen/standard, to minimize er-
maximum attained temperature. By testing an unknown speci- rors from pulse energy variations.
men after this calibration, the specific heat capacity can be
X2.2 The specimens density may be calculated from results
calculated from its maximum attained temperature, relative to
of weight measurements and computed volume. It is appropri-
the one obtained for the standard. There are several conditions
ate to calculate the density at each temperature from the room
that must be satisfied in order for this process to be valid:
temperature density, using thermal expansion data. Consult
X2.1.1 The energy source must be able to reproduce within
Test Method E228 for details.
5 % the energy of a pulse based on the power defining
parameter (charge voltage for lasers, for example) over a X2.3 Thermal conductivity may be calculated using Eq
period of time. X2.1, from the measured values of thermal diffusivity, specific
X2.1.2 The detector must maintain its sensitivity over a heat capacity and density.
period of time without drift, gain change, and within a linear X2.3.1 When measured values of specific heat capacity are
response range. used, the constrains listed under X2.1.1 X2.1.6 also apply to
X2.1.3 The reference specimen and the unknown specimen the resultant thermal conductivity.
must be very similar in size, proportions, emissivity, and X2.3.2 It is permissible to use specific heat capacity and
opacity, to approximate adiabatic behavior to the same extent. density data from other sources than the measurements above.
Both the reference and the unknown specimen should be
coated with a thin uniform graphite layer, to ensure that the X2.4 Reporting specific heat capacity or thermal conductiv-
emissivity of the two materials is the same. ity obtained in this manner must be accompanied by:

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X2.4.1 An accuracy statement determined; X2.4.3 Reference material used.
X2.4.2 The time elapsed between reference and test pulses;

X3. REFERENCE MATERIALS

X3.1 Only a few Standard Reference Materials (SRM) are 298 to 1025 K. Its certificate lists an uncertainty of 6 6 %. The
available from the National Metrology Institutes for thermal thermal diffusivity value is determined from the equation:
diffusivity. However, a large amount of data is available in the
~~ mm! 2 s 21 ! 54.406 2 1.35
literature on a number of industry-accepted reference materials
that have been used for verification purposes. 31022 T12.133
31025 T 2 2 1.541 (X3.1)
X3.1.1 A valuable summary and data bank of thermal 31028 T 3 14.147
diffusivity values found in the literature that also provides
310212T 4
recommended values for a wide range of materials, is also
available (20). where T is in K.

X3.2 A glass-ceramic thermal diffusivity standard reference


material, BCR-724,5 is available for the temperature range of

5
The sole source of supply of BCR-724 known to the committee at this time is
theInstitute for Reference Materials and Measurements, Retiesweg 11, B-2440 Geel,
Belgium, jrcirmm-rm-sales@ec.europa.eu. If you are aware of alternative suppliers,
please provide this information to ASTM International Headquarters. Your com-
ments will receive careful consideration at a meeting of the responsible technical
committee,1 which you may attend.

REFERENCES

(1) Parker, W. J., Jenkins, R. J., Butler, C. P., and Abbott, G. L., Flash P. H., ed., Plenum Publishing Corp., NY, 1974, p. 287. See also
Method of Determining Thermal Diffusivity Heat Capacity and Sweet, J. N., Data Analysis Methods for Flash Diffusivity
Thermal Conductivity, Journal of Applied Physics, Vol 32, 1961, pp. Experiments, Sandia National Laboratory Report SAND 89-0260,
16791984. (Available from NTIS), February, 1989.
(2) Watt, D. A., Theory of Thermal Diffusivity of Pulse Technique, (12) Clark, L. M., III, and Taylor, R. E., Radiation Loss in the Flash
British Journal of Applied Physics, Vol 17, 1966, pp. 231240. Method for Thermal Diffusivity, Journal of Applied Physics, Vol 46,
(3) Righini, F., and Cezairliyan, A., Pulse Method of Thermal Diffusivity 1975, pp. 714719.
Measurements, A Review, High TemperaturesHigh Pressures, Vol (13) Cowan, R. D., Pulse Method of Measuring Thermal Diffusivity at
5, 1973, pp. 481501. High Temperatures, Journal of Applied Physics, Vol 34, 1963, pp.
(4) Taylor, R. E., Heat Pulse Diffusivity Measurements, High 926927.
TemperaturesHigh Pressures, Vol 11, 1979, pp. 4358. (14) Larson, K. B., and Koyama, K., Measurement of Thermal
(5) Taylor, R. E., Critical Evaluation of Flash Method for Measuring Diffusivity, Heat Capacity and Thermal Conductivity in Two-Layer
Thermal Diffusivity, Revue Internationale des Hautes Temperatures Composite Samples by the Flash Method, in Proceedings 5th
et des Refractaires, Vol 12, 1975, pp. 141145. Thermal Conductivity Conference, University of Denver, Denver,
(6) Taylor, B. N., Kuyatt, C. E., Guidelines for Evaluating and Express- CO, 1965, pp. 1-B-1 to 1-B-24.
ing the Uncertainty of NIST Measurements Results, NIST Technical (15) Fitzer, Thermal Properties of Solid Materials, Project Section II
Note 1297, Gaithersburg, MD, 1994. Cooperative Measurements of Heat Transport Phenomena of Solid
(7) Cape, J. A., and Lehman, G. W., Temperature and Finite Pulse-Time Materials at High Temperatures, Advisory Group for Aerospace
Effects in the Flash Method for Measuring Thermal Diffusivity, Research and Development (AGARD), North Atlantic Treaty
Journal of Applied Physics, Vol 34, 1963, pp. 19091913. Organization, AGARD Report No. 606, 1973.
(8) Taylor, R. E., and Clark, III, L. M., Finite Pulse Time Effects in Flash (16) Carslaw H. S., and Jeager, J. C., Conduction of Heat in Solids, 2nd
Diffusivity Method, High TemperaturesHigh Pressures, Vol 6, ed., Oxford University Press, London, 1959.
1974, pp. 6572. (17) Taylor, R. E., and Cape, J. A., Finite Pulse-Time Effects in the Flash
(9) Larson, K. B., and Koyama, K., Correction for Finite Pulse-Time Diffusivity Technique, Applied Physics Letters, Vol 5, 1964, pp.
Effects in Very Thin Samples Using the Flash Method of Measuring 210212.
Thermal Diffusivity, Journal of Applied Physics, Vol 38, 1967, pp. (18) Azumi, T., and Takahashi, Y., Novel Finite Pulse-Width Correction
465474. in Flash Thermal Diffusivity Measurement, Review of Scientific
(10) Heckman, R. C., Error Analysis of the Flash Thermal Diffusivity Instruments, 1981, pp. 14111413.
Technique, Thermal Conductivity 14, Klemens, P. G., and Chu, T. (19) Mackay, J. A., and Schriempf, J. T., Corrections for Nonuniform
K., eds. Plenum Publishing Corp., NY, 1974, pp. 491498. Surface Heating Errors in Flash-Method Thermal Diffusivity
(11) Sweet, J. N., Effect of Experimental Variables on Flash Thermal Measurements, Journal of Applied Physics, Vol 47, 1976, pp.
Diffusivity Data Analysis, Thermal Conductivity 20, Hasselman, D. 16681671.

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E1461 13
(20) Touloukian, Y. S., Powell, R. W., Ho, C. Y., and Nicolaou, M.,
Thermal Diffusivity, Thermophysical Properties of Matter, Vol 10,
IFI/Plenum, NY, 1973.

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the Uncertainty of Measurement in Calibration, Edition 1, April Diffusivity of Layered Composites, Thermal Conductivity 15,
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(15) ISO Guide to the Expression of Uncertainty in Measurement. Lancaster, 1999.

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E1461 13
(30) Thermitus , M. A., and Gaal, P. S., Specific Heat Capacity of Some (32) Wang, H., Dinwiddie R. B., and Gaal, P. S., Multiple Station
Selected Materials with the Laser Flash Method, in Proceedings of Thermal Diffusivity Instrument, in Thermal Conductivity 23,
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